A New Two-Dimensional Molybdenum(V) Nickel Phosphate Built Up of [H<sub>18</sub>(Mo<sub>16</sub>O<sub>32</sub>)Ni<sub>16</sub>(PO<sub>4</sub>)<sub>26</sub>(OH)<sub>6</sub>(H<sub>2</sub>O)<sub>8</sub>]<sup>18-</sup> Wheels
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The new molybdenum(V) nickel phosphate Na6Ni6[(Mo2O4)8Ni16(H2PO4)4(HPO4)10(PO4)12(OH)6(H2O)8]·66H2O (1) was synthesized hydrothermally. The structure (orthorhombic, space group Cccm; a = 23.999(4), b = 36.595(6), c = 20.445(4) Å) was solved from single-crystal data. The framework structure of 1 consists of anionic inorganic sheets formed by the linkages of large polyoxomolybdate rings via nickel(II) octahedra. Charge-compensating sodium atoms are interleaved between the sheets. Magnetic studies of compound 1 revealed that among the 22 nickel(II) centers, 10 are interacting. The χMT = f(T) curve can be fitted using the dinuclear expression appropriate to the HDVV isotropic exchange Hamiltonian H = −2JS1·S2, with S1 = S2 = 1 and J = −24.1 cm-1, showing that nickel is antiferromagnetically coupled within Ni2 pairs.
